CN113552150A - 一种用于尿素检测及电解氧化的镍基催化剂 - Google Patents
一种用于尿素检测及电解氧化的镍基催化剂 Download PDFInfo
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Abstract
本发明提供一种用于尿素检测及电解氧化的镍基催化剂,所述镍基催化剂通过将双氰胺和镍盐混合后,高温反应制得。所述镍基催化剂是一种镍纳米颗粒嵌入氮掺杂的竹节碳纳米管的镍基催化剂。本发明制备过程简单,成本较低,适合大规模的生产,且制备的镍基催化剂催化活性好。
Description
技术领域
本发明涉及化学材料技术领域,涉及一种用于尿素检测及电解氧化的镍基催化剂,具体来说,涉及一种镍基催化剂及其制备方法和应用。
背景技术
化工厂生产排除的工业废水、农业生产造成的废水以及城市废水中均含有大量的尿素,未经任何处理直接排放则会造成水体污染,影响自然界的水体循环,对土壤和人类健康造成伤害。对含氮成分的污水采用合理办法进行净化处理,在环境和工业领域有重大意义。
传统的尿素处理方式包括水解、吸附、生物降解和化学氧化等,但这些方法所需设备的高成本以及过度能量消耗限制了其大规模应用。相较之下,将尿素氧化的反应(UOR)直接转化为电响应,能够很好避免上述问题;电响应运行简单,且产物稳定、无毒(CO2,N2和H2);更重要的是,除贵金属对尿素的氧化过程具有高活性外,部分过渡金属也可以有效地实现碱性条件下的尿素电氧化反应,很大程度上降低了催化剂的成本。研究表明:与其他金属催化剂相比,镍基催化剂具有更高的UOR活性,且三价镍(Ni3+)被证实为活性中心,因此,当前阳极催化剂的研究重点主要集中于镍基金属。
制备的镍基金属材料,首先存在的就是电流密度较小的问题,由于UOR发生在电极的三相界面上,因此催化剂的结构和形貌对其电化学性能有重要的影响;现有研究表明:低维纳米结构具有暴露的晶体表面和高比表面积,以提供更多反应活性位点,能提高尿素氧化的性能。纯的金属镍催化剂催化尿素氧化往往具有材料稳定性差的缺点,难以长时间的进行电氧化过程,在催化剂材料制备过程中,使用导电性好、比表面积大、好的化学稳定性的支撑材料能提高催化剂的耐久性和催化活性,例如:石墨烯,碳纳米管等能有效的提高金属催化剂的催化活性并且能减少金属的载量。
目前,大量的镍基纳米材料被制备出来,这些材料能有效的提高尿素氧化的催化活性,应用前景较好。但是除了性能良好之外,在材料合成中仍有一些问题亟待解决,例如制备过程繁琐,成本较高,不适合大规模的生产等等,这些都限制了催化剂在催化尿素氧化方面的实际应用。
针对相关技术中的问题,目前尚未提出有效的解决方案。
发明内容
针对相关技术中的上述技术问题,本发明提出一种用于尿素检测及电解氧化的镍基催化剂,其制备过程简单,成本较低,适合大规模的生产,且制备的镍基催化剂催化活性好。
为实现上述技术目的,本发明的技术方案是这样实现的:
一方面,本发明提供一种镍基催化剂,其特征在于,其为镍纳米颗粒嵌入氮掺杂的竹节碳纳米管的镍基催化剂。
进一步地,所述镍纳米颗粒位于所述竹节碳纳米管的末端。
进一步地,所述镍基催化剂的X-射线衍射图具有包括衍射角2θ在:26.2°、44.5°、51.8°、76.3°的衍射峰。
进一步地,所述镍基催化剂具有基本上如图3所示的X射线粉末衍射图。
进一步地,所述镍基催化剂的形貌具有基本上如图1所示的扫描电镜图。所述镍基催化剂结构是直径为40~200nm的纳米管,催化剂中镍纳米颗粒的平均粒径50nm。
一方面,本发明提供一种镍基催化剂的制备方法,步骤为:双氰胺和镍盐混合后,在高温作用下,双氰胺先热解,同时镍盐受热转变为金属单质,镍盐不仅作为热解催化剂将含碳有机物在高温下催化热解,也作为生长催化剂使得热解产生的碳原子沉积于催化剂表面,随后逐层生长为碳管,直至催化剂颗粒失活。
进一步地,所述镍盐为无机镍盐,进一步地,所述无机镍盐选自硝酸镍。
进一步地,所述镍盐中Ni与双氰胺中N的摩尔比为1:9~1:21。进一步地,所述Ni:N的摩尔比优选为1:14、1:9、1:21。
进一步地,所述高温反应在惰性气氛中进行。进一步地,所述惰性气氛为氩气气氛。
进一步地,所述高温反应的具体过程为:将双氰胺、镍盐混合后,在氩气气氛中,以5~20℃/min的升温速率加热到700~900℃,保持1~5小时。
进一步地,所述高温反应的具体过程为:将双氰胺、镍盐混合后,在氩气气氛中,以10℃/min的升温速率加热到700~900℃,保持2小时。
另一方面,本发明提供一种镍基催化剂在制备用于尿素检测及电解氧化废水中尿素的镍基催化剂中的应用。
本发明的有益效果:
本发明提供一种镍基催化剂及其制备方法和应用,解决现有技术中尿素氧化催化剂存在的氧化活性低、结构稳定性差、合成条件复杂等问题,实现采用简易的催化热分解法合成具有高催化氧化活性、良好耐久性的镍基催化剂。
本发明通过将硝酸镍作为镍源和生长催化剂,双氰胺作为碳源和氮源,混合后,在氩气氛围中经过高温(800℃)煅烧即可得到镍纳米颗粒嵌入氮掺杂的碳纳米管(Ni-NCNT)的镍基催化剂。所述镍基催化剂中,碳纳米管的表现形式为一维中空管材料,镍纳米粒子嵌入碳纳米管,构成复合材料。其中的碳纳米管具有良好的导电性且机械稳定,有利于电子传输并有独特的催化性能;通过将镍纳米粒子嵌入碳纳米管后形成的复合材料,可以在持续氧化条件下增强材料的稳定性和耐腐蚀性。
本发明制备的复合材料中,镍纳米颗粒位于CNTs的顶端,避免金属镍的团聚,并有利于活性位点的充分暴露,实验结果表明:适当的氮掺入有利于促进金属Ni电化学转化为活性Ni3+。
相比纯镍的电催化剂,由于N掺杂促进了活性Ni3+的转化,本发明制备的镍基催化剂对尿素的氧化效果大大提升;通过将镍负载在碳纳米管上赋予催化剂更优的尿素氧化性能;具有良好的稳定性;在催化过程中,由于镍复合碳载体后,加速氧化电解的反应动力学。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1本发明较优实施例制备的镍基催化剂的扫描电镜图
图2图1所述的镍基催化剂的透射电镜图
图3本发明制备的镍基催化剂的X-射线粉末衍射图
图4为催化剂在1mol KOH的电解液中LSV曲线,图中1.38V与1.4V处为金属Ni氧化为Ni3+的氧化峰,负载在氮掺杂的碳纳米管(NCNT)上的镍基催化剂比纯镍催化剂的氧化峰电流强度大,且氧化峰电位更小,说明N掺杂促进了活性物种Ni3+的转化,这将大大提升尿素的氧化效果。
图5为催化剂在含有0.33M尿素的1mol KOH中LSV曲线,加入尿素后氧化电流明显变大,说明合成的镍基催化剂均有良好的催化氧化效果,对比纯镍催化剂,负载在碳纳米管上后赋予催化剂更优的UOR性能。
图6为催化剂在含有0.33M尿素的1mol KOH中电流密度为10mA/cm-2时的恒电流曲线,经过15小时的氧化电解后,相比于纯镍,在NCNT保护下Ni-NCNT电解电压未发生明显升高,说明具有良好的稳定性。
图7为0.45V电压催化剂的交流阻抗曲线,镍复合碳载体后阻抗减小,电子转移能力提高,有利于加速氧化电解的反应动力学。
图8为每隔30s向电解液中添加0.1mM尿素的计时电流曲线,每次加入尿素溶液后氧化电流会迅速升高。
图9为计时电流曲线中电解液的尿素浓度与氧化产生的电流密度的线性拟合曲线,根据拟合曲线斜率可知催化剂检测和氧化尿素时的灵敏度为131.53uA/mM·cm2,表明合成的催化剂不仅可以用于处理污水,还可以用于水体中微量尿素成分的检测。
图10为实施例1制备的镍基催化剂的扫描电镜图
图11为实施例2制备的镍基催化剂的扫描电镜图
图12为实施例3制备的镍基催化剂的扫描电镜图
图13为实施例4制备的镍基催化剂的扫描电镜图
图14为实施例1~4制备的镍基催化剂的UOR性能对比图。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员所获得的所有其他实施例,都属于本发明保护的范围。
为了方便理解本发明的上述技术方案,以下通过具体使用方式上对本发明的上述技术方案进行详细说明。
实施例1
一种镍基催化剂的制备方法,步骤为:将双氰胺、镍盐混合后,在氩气气氛中,以10℃/min的升温速率加热到700℃,保持2小时反应制得;
所述镍盐中Ni与双氰胺中N的摩尔比为1:14。
所述镍盐选自:硝酸镍。
实施例2
一种镍基催化剂的制备方法,步骤为:将双氰胺、镍盐混合后,在氩气气氛中,以10℃/min的升温速率加热到800℃,保持2小时反应制得。所述镍盐中Ni与双氰胺中N的摩尔比为1:9。
所述镍盐选自:硝酸镍。
实施例3
一种镍基催化剂的制备方法,步骤为:将双氰胺、镍盐混合后,在氩气气氛中,以10℃/min的升温速率加热到800℃,保持2小时反应制得。
所述镍盐中Ni与双氰胺中N的摩尔比为1:21。
所述镍盐选自:硝酸镍。
实施例4
一种镍基催化剂的制备方法,步骤为:将双氰胺、镍盐混合后,在氩气气氛中,以10℃/min的升温速率加热到900℃,保持2小时反应制得。
所述镍盐中Ni与双氰胺中N的摩尔比为1:9。
所述镍盐选自:硝酸镍。
对比例
试验过程同实施例1,区别在于,将双氰胺替换为葡萄糖;制备得到纯镍的催化剂。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种镍基催化剂,其特征在于,其为镍纳米颗粒嵌入氮掺杂的竹节碳纳米管的镍基催化剂。
2.根据权利要求1所述的镍基催化剂,其特征在于,所述镍纳米颗粒位于所述竹节碳纳米管的末端。
3.根据权利要求1所述的镍基催化剂,其特征在于,所述镍基催化剂的X-射线衍射图具有包括衍射角2θ在:26.2°、44.5°、51.8°、76.3°的衍射峰。
4.根据权利要求1所述的镍基催化剂,其特征在于,所述镍基催化剂具有基本上如图3所示的X射线粉末衍射图。
5.根据权利要求1所述的镍基催化剂,其特征在于,所述镍基催化剂的形貌具有基本上如图1所示的扫描电镜图。
6.一种镍基催化剂的制备方法,其特征在于,步骤为:双氰胺和镍盐混合后,高温反应制得。
7.根据权利要求6所述镍基催化剂的制备方法,其特征在于,所述镍盐选自:硝酸镍。
8.根据权利要求6所述镍基催化剂的制备方法,其特征在于,所述镍盐中Ni与双氰胺中N的摩尔比为1:9~1:21。
9.根据权利要求6所述镍基催化剂的制备方法,其特征在于,所述高温反应的具体过程为:将双氰胺、镍盐混合后,在惰性气体气氛中,以5~20℃/min的升温速率加热到700~900℃,保持1~5小时。
10.一种权利要求1所述镍基催化剂在制备用于尿素检测及电解氧化废水中尿素的催化剂中的应用。
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